ASTM D5896-96

Standard Test Method for Carbohydrate Distribution of Cellulosic Materials

SCOPE
1.1 This test method covers the determination of the carbohydrate composition of cellulosic materials such as ground wood meal, chemically refined pulp, mechanical pulps, brownstocks, and plant exudates (gums) by ion chromatography. This test method is suitable for rapid, routine testing of large numbers of samples with high accuracy and precision. For a review of this technique, see Lee (1).
1.2 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For hazard statement, see Section 8.

General Information

• Status: Historical
• Publication Date: 31-Dec-2000
• Technical Committee: D01 - Paint and Related Coatings, Materials, and Applications
• Drafting Committee: D01.36 - Cellulose and Cellulose Derivatives

Relations

• Replaced By: ASTM D5896-96(2001) - Standard Test Method for Carbohydrate Distribution of Cellulosic Materials
• Effective Date: 01-Jan-2001

Standards Content (Sample)

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.
Designation: D 5896 – 96
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Carbohydrate Distribution of Cellulosic Materials
This standard is issued under the fixed designation D 5896; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.
1. Scope (5) ion chromatographic analysis, and
(6) calibration/calculation.
1.1 This test method covers the determination of the carbo-
hydrate composition of cellulosic materials such as ground
5. Significance and Use
wood meal, chemically refined pulp, mechanical pulps, brown-
5.1 This test method requires total hydrolysis of carbohy-
stocks, and plant exudates (gums) by ion chromatography. This
drate material to monosaccharides, and is thus applicable to
test method is suitable for rapid, routine testing of large
any cellulosic or related material that undergoes substantial
numbers of samples with high accuracy and precision. For a
2 hydrolysis, including cellulose derivatives such as cellulose
review of this technique, see Lee (1).
acetate.
1.2 This standard does not purport to address all of the
5.2 The carbohydrate composition of a cellulosic material
safety concerns, if any, associated with its use. It is the
can be expressed on the basis of the total initial sample, or on
responsibility of the user of this standard to establish appro-
the basis of the carbohydrate portion of the sample. The former
priate safety and health practices and determine the applica-
requires quantitative handling and may require special knowl-
bility of regulatory limitations prior to use. For hazard state-
edge of the other components present in order to establish the
ment, see Section 8.
absolute carbohydrate level or determine individual wood
2. Referenced Documents hemicelluloses such as galactoglucomannan, etc. Since the
solid portion of purified pulps is almost all carbohydrate
2.1 ASTM Standards:
(98 + %), the latter basis is often used to express the carbo-
D 1193 Specification for Reagent Water
hydrate distribution as a percent.
D 1695 Terminology of Cellulose and Cellulose Deriva-
5.3 If heated under alkaline conditions, isomeric sugars may
tives
begin to appear in the chromatogram. The major impurity
3. Terminology
present in purified pulps is saccharinic acids. These acidic
components, and other anions such as sulfate, carbonate, and
3.1 For standard terminology of cellulose and cellulose
acetate are removed by a strong base anion exchange SPE, and
derivatives, see Terminology D 1695.
would need to be determined separately to get a more exact
3.2 Abbreviations:
carbohydrate distribution.
3.2.1 IC—ion chromatography,
3.2.2 SPE—solid phase extraction,
6. Apparatus
3.2.3 PAD—pulsed amperometric detector,
6.1 Blender.
3.2.4 PED—pulsed electrochemical detector,
6.2 Screw Cap Culture Tubes, 25 by 150 mm, outside
3.2.5 mM—millimolar.
diameter.
4. Summary of Test Method
6.3 Refrigerator.
6.4 Pressure Cooker.
4.1 IC analysis of cellulosics requires the following opera-
6.5 SPE Cartridges.
tions:
6.6 Water Bath.
(1) sample preparation,
6.7 Ion Chromatograph.
(2) total hydrolysis,
6.8 Moisture Balance.
(3) dilution,
6.9 Hot Plate.
(4) SPE,
6.10 Pipets.
This test method is under the jurisdiction of ASTM Committee D-1 on Paint
TOTAL HYDROLYSIS
and Related Coatings, Materials, and Applicationsand is the direct responsibility of
Subcommittee D01.36on Cellulose and Cellulose Derivatives.
7. Reagents and Materials
Current edition approved Jan. 10, 1996. Published March 1996.
The boldface numbers in parentheses refer to the list of references at the end of
7.1 Sulfuric Acid (72 6 0.1 weight %): To 1 volume of
this test method.
water, add slowly while stirring vigorously 2 volumes of
Annual Book of ASTM Standards, Vol 11.01.
4 concentrated sulfuric acid (sp gr 1.84). Standardize against an
Annual Book of ASTM Standards, Vol 06.03.
D 5896
alkaline standard, and adjust to 72 6 0.1 weight %. sembled from the individual components, or purchased as a
system.
12.2 Column—The column must be suitable for separating
8. Hazards
monosaccharides and is generally protected by a suitable guard
8.1 Precaution: Wear eye protection and chemical resistant
column. A column packing material that works well is com-
gloves while working with strong acid.
posed of 10 μm beads of surface-sulfonated polystyrene/
divinylbenzene (2 % crosslinked), covered with porous latex
9. Summary of Procedure
beads containing alkyl quaternary amine functionality.
9.1 The total hydrolysis of cellulosic material requires a
13. Procedure
primary hydrolysis with strong mineral acid followed by a
13.1 Perform the analysis using an ion chromatograph.
secondary hydrolysis in dilute acid. The primary hydrolysis
13.2 Inject 100 μL of sample onto the analytical column.
results in the formation of a mixture of oligosaccharides; the
13.3 Detection is by PAD or PED in a pulsed amperometric
secondary hydrolysis completes the conversion to monomeric
mode using a gold working electrode.
sugars.
13.4 Standard pulp samples are generally run isocratically at
1 mL/min using an eluant of 2.5 mM sodium hydroxide to
10. Sampling, Test Specimens, and Test Units
obtain baseline resolution of fucose (internal standard), arabi-
10.1 Extract wood samples with ethanol to remove extrac-
nose, galactose, glucose, xylose, and mannose in less than 30
tives, then grind in a Wiley mill to pass a 40-mesh screen.
min. If other sugars are present, it may be necessary to alter the
Disintegrate (fluff) dry pulp or paper samples in a blender.
eluant strength, or try a gradient approach.
Determine the moisture content using a moisture balance or
13.5 Eluant is degassed and kept under helium (nitrogen
similar device.
may be substituted for helium).
13.6 A 0.5-mL/min flow of 0.3-M NaOH is added after the
11. Procedure
column,
...